With decreasing system sizes, the mechanical properties and dominant deformation mechanisms of metals change. For larger scales, bulk behavior is observed that is characterized by a preservation and significant increase of dislocation content during deformation whereas at the submicron scale very localized dislocation activity as well as dislocation starvation is observed. In the transition regime it is not clear how the dislocation content is built up. This dislocation storage regime and its underlying physical mechanisms are still an open field of research. In this paper, the microstructure evolution of single crystalline copper micropillars with a $\langle1\,1\,0\rangle$ crystal orientation and varying sizes between $1$ to $10\,μ\mathrm{m}$ is analysed under compression loading. Experimental in situ HR-EBSD measurements as well as 3d continuum dislocation dynamics simulations are presented. The experimental results provide insights into the material deformation and evolution of dislocation structures during continuous loading. This is complemented by the simulation of the dislocation density evolution considering dislocation dynamics, interactions, and reactions of the individual slip systems providing direct access to these quantities. Results are presented that show, how the plastic deformation of the material takes place and how the different slip systems are involved. A central finding is, that an increasing amount of GND density is stored in the system during loading that is located dominantly on the slip systems that are not mainly responsible for the production of plastic slip. This might be a characteristic feature of the considered size regime that has direct impact on further dislocation network formation and the corresponding contribution to plastic hardening.
Based on the cross correlation analysis of the Kikuchi diffraction patterns high-resolution EBSD is a well established method to determine the internal stress in deformed crystalline materials. In many cases, however, the stress values obtained at the different scanning points have a large (in the order of GPa) scatter. As it was first demonstrated by Wilkinson and co-workers this is due to the long tail of the probability distribution of the internal stress ($P(σ)$) generated by the dislocations present in the system. According to the theoretical investigations of Groma and co-workers the tai…
The mechanical behavior in compression of [111] LiF micropillars with diameters in the range 0.5 $μ$m to 2.0 $μ$m was analyzed by means of discrete dislocation dynamics at ambient and elevated temperature. The dislocation velocity was obtained from the Peach-Koehler force acting on the dislocation segments from a thermally-activated model that accounted for the influence of temperature on the lattice resistance. A size effect of the type "smaller is stronger" was predicted by the simulations, which was in quantitative agreement with previous experimental results by the authors \cite{SWC14}. Th…
Temperature-activated dislocation avalanches signaling brittle-to-ductile transition in BCC micropillars
School of Mechanics & Engineering Science, Shanghai University（上海大学力学与工程科学学院）；Department of Mechanical & Aerospace Engineering, University of Miami（迈阿密大学机械与航空航天工程系）；School of Physics, Sun Yat-sen University（中山大学物理学院）；Department of Mechanical & Aerospace Engineering, University of California Los Angeles（加州大学洛杉矶分校机械与航空航天工程系）
The μ-phase is a common precipitation phase in superalloys and it exists in a wide composition and temperature range. As such, we study the influences of composition and temperature on its plasticity by micropillar compression tests and transmission electron microscopy. The micropillars of the μ-Co7Nb6 phase deform plastically by basal slip at either room temperature or 600 oC. At room temperature, the Co-49Nb and Co-52Nb micropillars show high yield stresses and an abrupt large strain burst at the onset of yielding regardless of orientation, whereas the Co-54Nb micropillars oriented for basal…
The dislocation microstructure developing during plastic deformation strongly influences the stress-strain properties of crystalline materials. The novel method of high resolution electron backscatter diffraction (HR-EBSD) offers a new perspective to study dislocation patterning. In this work copper single crystals deformed in uniaxial compression were investigated by HR-EBSD, X-ray line profile analysis, and transmission electron microscopy (TEM). With these methods the maps of the internal stress, the Nye tensor, and the geometrically necessary dislocation (GND) density were determined at di…
High angular resolution electron backscatter diffraction (HR-EBSD) was coupled with focused ion beam (FIB) slicing to characterize the shape of the plastic zone in terms of geometrically necessary dislocations (GNDs) in W single crystal in 3 dimensions. Cantilevers of similar size with a notch were fabricated by FIB and were deformed inside a scanning electron microscope at different temperatures (21$^{\circ}$C, 100$^{\circ}$C and 200$^{\circ}$C) just above the micro-scale brittle-to-ductile transition (BDT). J-integral testing was performed to analyse crack growth and determine the fracture t…
The plastic deformation mechanisms of tungsten carbide at room and elevated temperatures influence the wear and fracture properties of WC-Co hardmetal composite materials. The relationship between residual defect structures, including glissile and sessile dislocations and stacking faults, and the slip deformation activity, which produce slip traces, is not clear. Part 1 of this study showed that {10-10} was the primary slip plane at all measured temperatures and orientations, but secondary slip on the basal plane was activated at 600 °C, which suggests that <a> dislocations can cross-slip onto…
Plastic deformation in microscale differs from the macroscopic plasticity in two respects: (i) the flow stress of small samples depends on their size (ii) the scatter of plasticity increases significantly. In this work we focus on the scatter of plasticity. We statistically characterize the deformation process of micropillars under tension using results from discrete dislocation dynamics (DDD) simulations. We then propose a stochastic microplasticity model which uses the extracted information from the above statistical characterization to make statistical predictions regarding the micropillar …
The mechanisms of dislocation/precipitate interaction as well as the critical resolved shear stress were determined as a function of temperature in a Mg-4 wt. % Zn alloy by means of micropillar compression tests. It was found that the mechanical properties were independent of the micropillar size when the cross-section was $>$ 3 x 3 $μ$m$^2$. Transmission electron microscopy showed that deformation involved a mixture of dislocation bowing around the precipitates and precipitate shearing. The initial yield strength was compatible with the predictions of the Orowan model for dislocation bowing a…
The Effect of Pattern Quality on Measurements of Stress Heterogeneity and Geometrically Necessary Dislocation Density by High-Angular Resolution Electron Backscatter Diffraction
Microcrystals deform very differently from their macroscopic counterparts, displaying a size-dependent yield stress and intermittent plastic strain bursts. Here we demonstrate that size effects and strain bursts may be just two different signatures of fundamental collective phenomena that govern the dynamics of dislocation systems on all scales. We confirm this conjecture by demonstrating agreement between the results of 2D and 3D dislocation dynamics simulations and experimental results on compressed micropillars. Our results indicate that many peculiarities of small-sample plasticity may ari…
The effect of Ca and Zn in solid solution on the critical resolved shear stress (CRSS) of <a> basal slip, tensile twinning and <c+a> pyramidal slip in Mg alloys has been measured through compression tests on single crystal micropillars with different orientations. The solute atoms increased the CRSS for basal slip to ~ 13.5 MPa, while the CRSS for pyramidal slip was lower than 85 MPa, reducing significantly the plastic anisotropy in comparison with pure Mg. Moreover, the CRSSs for twin nucleation and growth were very similar (~ 37 MPa) and the large value of the CRSS for twin growth hindered t…
Characterizing plasticity mechanisms below the ductile-to-brittle transition temperature is traditionally difficult to accomplish in asystematic fashion. Here, we use a new experimental setup to perform in situ cryogenic mechanical testing of pure Sn micropillars at room temperature and at 142°C. Subsequent electron microscopy characterization of the micropillars shows a clear difference in the deformation mechanisms at room temperature and at cryogenic temperatures. At room temperature, the Sn micropillars deformed through dislocation plasticity, while at142°C they exhibited both higher stren…
Metals are important structural materials for transport and the built environment. Low carbon steels can fail through strain localisation due to the role of interstitial solute atoms (such as carbon and nitrogen) interacting with mobile dislocations, and this gives rise to the Portevin-Le Chatelier effect and the formation of Luders bands. In this work, we use in-situ tensile testing and observation with High Angular Resolution Electron Back Scatter Diffraction (HR-EBSD) to explore deformation patterning in two Interstitial Free (IF) steel samples. One of these steels was heat treated to trigg…
Predicting the dramatic changes in material properties caused by irradiation damage is key for the design of future nuclear fission and fusion reactors. Self-ion implantation is an attractive tool for mimicking the effects of neutron irradiation. However, the damaged layer of implanted samples is only few microns thick, making it difficult to estimate macroscopic properties. Here we address this challenge using a combination of experimental and modelling techniques. We concentrate on self-ion-implanted tungsten, the front-runner for fusion armour components and a prototypical bcc material. To …
Compression experiments on micron-scale specimens and acoustic emission (AE) measurements on bulk samples revealed that the dislocation motion resembles a stick-slip process - a series of unpredictable local strain bursts with a scale-free size distribution. Here we present a unique experimental set-up, which detects weak AE waves of dislocation slip during the compression of Zn micropillars. Profound correlation is observed between the energies of deformation events and the emitted AE signals that, as we conclude, are induced by the collective dissipative motion of dislocations. The AE data a…
Analysis of distortions of the crystal lattice within individual mineral grains is central to the investigation of microscale processes that control and record tectonic events. These distortions are generally combinations of lattice rotations and elastic strains, but a lack of suitable observational techniques has prevented these components being mapped simultaneously and routinely in earth science laboratories. However, the technique of high-angular resolution electron backscatter diffraction (HR-EBSD) provides the opportunity to simultaneously map lattice rotations and elastic strains with e…
The mechanisms of dislocation/precipitate interactions were analyzed in an Al-Cu alloy containing a homogeneous dispersion of $θ'$ precipitates by means of discrete dislocation dynamics simulations. The simulations were carried out within the framework of the discrete-continuous method and the precipitates were assumed to be impenetrable by dislocations. The main parameters that determine the dislocation/precipitate interactions (elastic mismatch, stress-free transformation strains, dislocation mobility and cross-slip rate) were obtained from atomistic simulations, while the size, shape, spati…
The deformation behaviour of the intermetallic Al$_{2}$Cu-phase was investigated using atomistic simulations and micropillar compression, where slip on the unexpected {211} and {022} slip planes was revealed. Additionally, all possible slip systems for the intermetallic phases were further evaluated and a preference for the activation of slip systems based on their effective interplanar distances as well as the effective Burgers vector is proposed. The effective interplanar distance corresponds to the manually determined interplanar distance, whereas the effective Burgers vector takes a potent…
Detailed microstructure characterisation and in-situ micropillar compression were coupled with crystal plasticity-based finite element modelling (CP-FEM) to study the micro-mechanisms of plastic anisotropy in lamellar TiAl alloys. The consideration of microstructure in both simulation and in-situ experiments enables in-depth understanding of micro-mechanisms responsible for the highly anisotropic deformation response of TiAl on the intra-lamella and inter-lamella scales. This study focuses on two specific configurations of γ/α_2 lamellar microstructure with the γ/α_2 interfaces being aligned {…
Decoupling Strain-Rate Sensitivity and Deformation Length Scale Effects in Neutron-Irradiated Tungsten: A Coupled Nano-Indentation, HR-EBSD and Crystal Plasticity Study
Indian Institute of Science（印度科学学院）；University of Oxford（牛津大学）；UK Atomic Energy Authority（英国原子能管理局）
Plastic deformation of microsamples is characterised by large intermittent strain bursts caused by dislocation avalanches. Here we investigate how ion irradiation affects this phenomenon during single slip single crystal plasticity. To this end, in situ compression of Zn micropillars oriented for basal slip was carried out in a SEM. The unique experimental setup also allowed the concurrent recording of the acoustic emission (AE) signals emitted from the sample during deformation. It was shown that irradiation introduced a homogeneous distribution of basal dislocation loops that lead to hardeni…
We present a framework which unifies classical phenomenological $J_2$ and crystal plasticity theories with quantitative dislocation mechanics. The theory allows the computation of stress fields of arbitrary dislocation distributions and, coupled with minimally modified classical ($J_2$ and crystal plasticity) models for the plastic strain rate of statistical dislocations, results in a versatile model of finite deformation mesoscale plasticity. We demonstrate some capabilities of the framework by solving two outstanding challenge problems in mesoscale plasticity: 1) recover the experimentally o…
Experimentally-validated multi-slice simulation of electron diffraction patterns
School of Materials Science and Engineering, Xiangtan University（湘潭大学材料科学与工程学院）；SJTU-ParisTech Elite Institute of Technology, Shanghai Jiao Tong University（上海交通大学巴黎卓越工程师学院）；School of Materials Science and Engineering, Shanghai Jiao Tong University（上海交通大学材料科学与工程学院）；Université Paris-Saclay, ENS Paris-Saclay, CNRS, LMPS - Laboratoire de Mécanique Paris-Saclay（巴黎萨克雷大学、巴黎高等师范学校、法国国家科学研究中心、LMPS巴黎萨克雷力学实验室）
Plasticity in body-centred cubic (BCC) metals, including dislocation interactions at grain boundaries, is much less understood than in face-centred cubic (FCC) metals. At low temperatures additional resistance to dislocation motion due to the Peierls barrier becomes important, which increases the complexity of plasticity. Iron-silicon steel is an interesting, model BCC material since the evolution of the dislocation structure in specifically-oriented grains and at particular grain boundaries have far-reaching effects not only on the deformation behaviour but also on the magnetic properties, wh…
The use of Nye's dislocation tensor for calculating the density of geometrically necessary dislocations (GND) is widely adopted in the study of plastically deformed materials. The curl operation involved in finding the Nye tensor, while conceptually straightforward has been marred with inconsistencies and several different definitions are in use. For the three most common definitions, we show that their consistent application leads to the same result. To eliminate frequently encountered confusion, a summary of expressions for Nye's tensor in terms of elastic and plastic deformation gradient, a…
Plastic inhomogeneity, particularly localised strain, is one of the main mechanisms responsible for failures in engineering alloys. This work studied the spatial arrangement and distribution of microstructure and their influence in the plastic inhomogeneity of Inconel 718 fabricated by additive manufacturing (AM). In particular, the density and spatial distribution of geometrically necessary dislocations (GNDs) and the crystallographic texture components were examined in relation to the spatial plastic deformation. In-situ tensile testing coupled with microscopy and EBSD was performed to under…
It is now possible to create perfect crystal nanowires of many metals. The deformation of such objects requires a good understanding of the processes involved in plasticity at the nanoscale. Isotropic compression of such nanometre scale micropillars is a good model system to understand the plasticity. Here we investigate these phenomena using Molecular Dynamics (MD) simulations of nanometre scale single crystal BCC iron pillars in compression. We find that pillars with large length to width ratio may buckle under high strain rates. The type of buckling behaviour depends sensitively on the boun…
Zircaloy-4 is used extensively as nuclear fuel cladding materials and hydride embrittlement is a major failure mechanism. To explore the effect of δ-hydride on plastic deformation and performance of Zircaloy-4, in situ high angular resolution electron backscatter diffraction (HR-EBSD) was used to quantify stress and geometrically necessary dislocation (GND) density during bending tests of hydride-free and hydride-containing single crystal Zircaloy-4 microcantilevers. Results suggest that while the stress applied was accommodated by plastic slip in the hydride-free cantilever, the hydride-conta…
Multiphase titanium alloys are critical materials in high value engineering components, for instance in aero engines. Microstructural complexity is exploited through interface engineering during mechanical processing to realise significant improvements in fatigue and fracture resistance and strength. In this work, we explore the role of select interfaces using in-situ micromechanical testing with concurrent observations from high angular resolution electron backscatter diffraction (HR-EBSD). Our results are supported with post mortem transmission electron microscopy (TEM). Using micro-pillar c…
Molybdenum disilicide (MoSi$_2$) is a very promising material for high temperature structural applications due to its high melting point (2030 °C), low density, high thermal conductivity and good oxidation resistance. However, MoSi$_2$ has limited ductility below 900 °C due to its anisotropic plastic deformation behaviour and high critical resolved shear stresses on particular slip systems. Nanoindentation of MoSi$_2$ microalloyed with aluminium, niobium or tantalum showed that all alloying elements cause a decrease in hardness. Analysis of surface slip lines indicated the activation of the ad…
Creep of directionally solidified Sn-3Ag-0.5Cu wt.% (SAC305) samples with near-<110> orientation along the loading direction and different microstructural lengthscale is investigated under constant load tensile testing and at a range of temperatures. The creep performance improves by refining the microstructure, i.e. the decrease in secondary dendrite arm spacing (λ2), eutectic intermetallic spacing (λe) and intermetallic compound (IMC) size, indicating as a longer creep lifetime, lower creep strain rate, change in activation energy (Q) and increase in ductility and homogeneity in macro- and m…
A mesoscale study of a single crystal nickel-base superalloy subjected to an industrially relevant process simulation has revealed the complex interplay between microstructural development and the micromechanical behaviour. As sample gauge volumes were smaller than the length scale of the highly cored structure of the parent material from which they were produced, their subtle composition differences gave rise to differing work hardening rates, influenced by varying secondary dendrite arm spacings, gamma-prime phase solvus temperatures and a topologically inverted gamma/gamma-prime microstruct…
